Alkaline detergent powder and method of making the same



252. COMPOSITIONS,

Patented Mar. 17, 1936 UNITED STATES- Examine;

PATENT OFFICE Boy 0. Sutton, University City, Mo.

N Drawing.

Application March 23, 1929,

Serial No. 349,514

17 Claims.

This invention relates to alkaline detergents and methods of preparing the same. In certain industries wherein the use of detergents forms an essential part and wherein chlorine as a bleach or disinfectant has been desirable, it has been customary for the user to depend separately upon alkaline detergents and upon separate available or active chlorine. The chlorine serves primarily as a bleaching agent in the laundry, textile and similar industries and as a disinfectant in other uses, while the alkalis serve primarily as water softeners and detergents. The present practice in making use of chlorine may be defined as follows. If the source of chlorine is the so-called chloride of lime; that is, lime which has absorbed about thirty-three per cent. of its weight in chlorine, certain disadvantages have been met with. The chloride of lime tends to decompose; that is, to lose its active or available chlorine on exposure to air, and the chloride of lime has a very corrosive action on metallic containers. In addition to this fact, the lime must be removed from the composition when it is desired to use the chlorine for laundry purposes, due to the fact that the lime would form insoluble compounds with soap and would tend to harden the water. In this connection, it is one of the features of this invention that an alkaline detergent powder is afforded which is substantially free of lime or other alkaline earth which tends to harden water. The removal of the lime from the composition is troublesome and expensive, involving the addition of soda ash or a similar reagent before use. In some instances, use is made of chlorine in the form of a liquid soda or lime bleach, which must necessarily be handled in glassor rubber-lined containers. Such containers are very expensive, and the transportation costs of handling containers so filled with this mixture oftentimes exceed the value of the mixture itself. Moreover, it is necessary in the instance of the liquid lime bleach to have the lime removed before the compound can be used for laundry purposes.

If liquid chlorine is used, the difficulties encountered are those of handling a highly compressed poisonous gas which must be converted into a solution before use. This dissolving process, in addition to being a dangerous one, is one which involves considerable equipment and labor, a disadvantage apparent in the laundry and other industries. The electrolytic process of producing is to provide an alkaline detergent powder containing chlorine as a bleaching or sterilizing agent.

A further object of the invention is to provide 7 methods of preparing an alkaline detergent powder having chlorine as a bleaching or disinfecting agent.

According to the present invention, a powder is produced which may be used as a detergent and as a bleach for laundry and similar purposes and which may be used in other industries as a dis infectant as well as a detergent. The powder is composed principally of available ordc'ti've chlorine, free or active alkali in the nature of a detergent, and water which isv css ntial in the manufacture of the mixture. andwtgfst aiicfian absorptive material. which ai 1n formation of the powder. A powder of this composition; that is, composed of available or active chlorine, free or active alkaline detergents, and water,- may be readily transported in its natural state, may be used without further preparation in a laundry or other use wherein chlorine may be used to advantage, and, since it is in powdered form, the transportation costs are not excessive in proportion to the value of the product.

For detergent purposes, the following are generally used, alone or in combination:

so-called modified sodas, sodium silicate, caustic potash, potassium carbonates, etc., borax etc., and the term alkali used hereinafter for brevity is to be understood to cover any one of the above or a combination of any of the above ingredients or any other alkali metal compound or compounds having pronounced basic characteristics. Each of the above alkalis possesses some advantages and some disadvantages peculiar to itself. It has been found in practice that a powder suitable for laundry and similar purposes and for detergent and disinfectant purposes may be composed of available or active chlorine, free or active alkali, water and an absorptive material, such powder being alkaline in nature and free from fats, fatty acids, or oils, and fatty or oily substances as distinguished from so-called soaps and soap products. The proportions of ingredients used in the mixture may be fixed within the ranges of substantially as follows:

Available or active chlorine substantially 1 to 15 per cent;

gaseous chlorine at the place where the chlorine .J Free or active alkali substantially 30 to 90%;

is to be used has been abandoned practically on account of the high expense involved.

Accordingly, an object of the present invention er bstantially 15 to 40 per cent: bsorptive nd inert material, the balance. The powder may be made up in several ways,

' desired.

but the preferred methods of producing the same are substantially as follows.

Chlorin be passed into an aqueous solution of caustic soda under conditions of controlled temperature to form the customary soda bleach solution of the nature of sodium hypochlorite. This solution may then be thoroughly mixed w' h ash, the materials being used in such quantities that the final composition is composed of ingredients within the ranges set forth hereinabove. The material so produced is friable and may be reduced to suitable dere fineness, in which condition it may be used for laundry and similar purposes or for any purpose wherein the use of an alkaline detergent in connection with a bleach or sterilizing agent is In this form, however, the compound has the tendency to harden into a solid mass, be-

coming somewhat difficult and inconvenient to use after solidification.

For purposes of rendering the product more easily transportable and of a form more suitable, the compound produced in the above manner may be treated in one of the following ways. Into the mixture of soda ash and sodium hypochlorite, there may be mixed some inert absorptive mat lialsnchaslsi selammmnuwamnt'ities sufficient to absorb the moisture content of the solution. Such substancesajr'dsubstantiallywat'er-insoluble solids which in their finely-divided state mechanically absorb water present in the mixture thus inhibiting hydraulic setting due to chemical formation in the mass of crystals containing water of crystallization and fixing the sodium hypochlorite solution so as to relatively permanently retain its available chlorine content. The addition of this absorptive material renders the final product more friable and causes the compound, when reduced to powdered fineness, to hold this state. A second way of treating the mixture of soda ash and sodium hypochlorite is to introduce into the mixture gaseous chlorine. The introduction of gaseous chlorine renders the product more friable, permitting it to be powdered. In the use of this method of finally treating the composition with gaseous chlorine, it is to be understood that the chlorine content of tnemfilonre wm be such that the final product evolved by the addition to the mixture of gaseous chlorine will contain available chlorine within the range set forth hereinbefore as desirable.

A still further process of treating the mixture of soda ash and sodium hypochlorite is to introduce into this mixture gaseous carbon dioxide which likewise renders the final product more friable and permits it to be reduced to the desired powdered fineness.

A powder meeting the requirements of the invention can be produced by adding to the sodium hypochlorite, powdered alkali metal silicate forming a wet creamy mass which may then be stirred into soda ash resulting in a final product which can be reduced to a powder. The materials are used in such proportions as to ggsjnt in a final product' icjoptaiping ingredi'efits with: in the specifiedraj iges. If so Hearse; theprodiiTzf riiay'b'treated as before, either by the addition of the absorptive inert materials such as kieselguhr, bentonite, etc., or by the introduction of gaseous chlorine or gaseous carbon dioxide which, in either event, renders the product more friable and causes it to remain in powdered state after having been reduced thereto.

A still further process may be carried out by merated alkalis or any combination of such, 31-

kalis, the ingredients being used in such quantities as to produce, as before stated, a final product containing them in quantities within the specified ranges. This product likewise may be either reduced to powdered fineness in its present state, or further treated by the addition of the absorptive material, or by the influence of gaseous chlorine or gaseous carbon dioxide.

A still further process may be used to produce a powder of the desired form by dissolving caustic soda in an appropriate quantity of water; thoroughly mixing the solution so formed with the dry alkali desired under controlled temperature conditions; and then introducing thereinto gaseous chlorine. As before stated, the

ingredients should be used in such quantities 3 that the final product will be made up of the ingredients within the specified ranges.

A mixture made up in the following manner has been found in practice to produce as a final product a powder which contains available or active chlorine, free or active alkali, and water, these ingredients being within the ranges hereinbefore set forth. Sodium hypochlorite is made up as follows: 18 pounds of caustic soda may be dissolved in 82 pounds of water and to this 15 pounds of chlorine are addedmaking ahypochlorite solution containing not more than about fifteen per cent. available chlorine. To itlggunds of spdagash there are added 5J2Ql1nds of silicate of .aeda 25 p ds .Qt..ths a 1dium ln299h 9ri ready produced, and 6 pounds of kieselguhr or bentonite or other absorptive materials. The

"resiiltingfifi pounds of mixture contain approximately 58 per cent. soda ash, 6 per cent. silicate of soda, 7 per cent. kieselguhr, 4 per cent. chlorine, 20 per cent. water and 5 per cent. inert material resulting from chemical reaction. Reduced to simpler terms, the mixture contains approximately 4 per cent. active chlorine, 64 per cent. active alkali, 20 per cent. water, and 12 per cent. inert material and absorptive material. The product so produced is friable and may be reduced to a finely-powdered state available for use and is easily transportable.

A powder meeting the terms of the invention may be also produced in the following manner: To 2g pounds gf soda ash there are added 25 moundmofntii-samnmflnhnsnbate, jnpounds of r a. 8 and Z mund s ols odi urn hypochlorite produced as above described. The powder resulting from this mixture of weight of 88 pounds is found to contain approximately 28 per cent. soda ash, 6 per cent. siicate of soda, 9 per cent. kieselguhr, 20 per cent. water (derived from the sodium hypochlorite), 28 per cent. tri-sodium phosphate, 4 per cent. chlorine, and 5 per cent. inert material resulting from chemical reaction. Reduced to simpler terms, the mixture contains approximately 4 per cent. active chlorine, 62 per cent.

ZOL.

active alkali, per cent. water, and 14 per cent. inert material and absorptive material.

A still further formula may be utilized for producing a powder falling within the terms of the invention: To 30 pounds of soda ash there are added 14 pounds of tri-sodium phosphate, 3 pounds of caustic soda, 5 pounds of silicate of soda, 10 pounds of kieselguhr or its equivalent, and pounds of sodium hypochlorite, producing approximately 87 pounds of powdered material. In this powder, there are approximately 34 per cent. soda ash, 16 per cent. tri-sodium phosphate, 4 per cent. caustic soda, 6 per cent. silicate of soda, 11 per cent. kieselguhr, 4 per cent. chlorine, 20 per cent. water (derived from the sodium hypochlorite), and 5 per cent. inert material resulting from chemical reaction. Reduced to simpler terms, the powder contains approximately 4 per cent. active chlorine, 60 per cent. active alkali, 20 per cent. water, and 16 per cent. inert material and absorptive material.

From the foregoing, it will be seen that the present invention provides methods of making a new powder which is in the nature of an alkaline detergent containing available or active chlorine, which powder may be used advantageously for laundry and similar purposes and may also be used for detergent purposes wherein a disinfectant is desired at the same time. Due to the fact that the material is in a powdered form and maintains this form, it is readily transportable and furthermore it obviates the necessity of mixing the ingredients by the user at the time of use, since the contents of this new mixture can be accurately gauged and determined.

Throughout the description relative to the invention, the chlorine used therein has been described as available or active chlorine, and it is to be understood that these terms as used herein are synonymous, and should be so considered wherever used. Likewise, the terms free or active as applied to alkali are synonymous and should be so considered. It is to be understood furthermore that the invention is not to be limited by the described embodiments, but is to be limited only by the scope of the following claims.

I claim:

1. An alkaline detergent powder substantially free of alkaline earth comprising alkali-metal hypochlorite solution which imparts to the powder available chlorine in the proportion of substantially 1% to 15%, alkali metal compound having alkaline characteristics in the proportion of substantially to 90%,, water in the proportion of substantially 15% to and finely-divided solid substantially-inert substantially-water-insoluble inorganic water-absorptive material to absorb excess moisture.

2. An alkaline detergent powder comprising sodium hypochlorite which imparts to the powder approximately 4% available chlorine, approximately 62% free alkali selected from the group consisting of alkali metal hydroxides, carbonates and phosphates, approximately 20% water and a finely-divided solid substantially inert substantially-water-insoluble water-absorptive material.

3. An alkaline detergent powder comprising sodium hypochlorite which imparts to the powder approximately 4% available chlorine, approximately 62% free alkali selected from the group consisting of alkali metal carbonates, phosphates, silicates and borates, approximately 20% water and inert water-absorptive material selected from the group consisting of kieselguhr and bentonite.

4. A friable alkaline detergent powder comprising a crystalline water-soluble alkaline alkali metal compound containing water of crystallization, a finely-divided solid substantially-inertsubstantially-water-insoluble water absorptive material distributed throughout and interspersed between the crystals of said alkaline alkali metal compound, and alkali-metal hypochlorite solution having available chlorine, said hypochlorite solution being absorbed by said water-absorptive material, said powder containing substantially one per cent. to fifteen per cent. available chlorine, substantially thirty per cent. to ninety per cent. alkali metal compound, and substantially fifteen per cent. to forty per cent. water.

5. A friable alkaline detergent powder comprising a crystalline water-soluble alkaline alkali metal compound containing water of crystallization, a finely-divided solid substantially-inert substantially-water-insoluble water absorptive material distributed throughout and interspersed between the crystals of said alkaline alkali metal compound, and alkali-metal hypochlorite solution having available chlorine, said hypochlorite solution being absorbed by said water absorptive material, said powder containing about four per cent. available chlorine, about sixty-two per cent. free alkali, and about twenty per cent. water.

6. A friable alkaline detergent powder substantially free of a water hardening alkaline earth compound comprising a crystalline water-soluble alkaline alkali metal compound containing water of crystallization, a finely-divided solid substantially-inert substantially-water-insoluble water-absorptive material selected from the group consisting of kieselguhr and bentonite clay distributed throughout and interspersed between the crystals of said alkaline alkali metal compound, and sodium hypochlorite solution having available chlorine, said sodium hypochlorite solution being absorbed by said water-absorptive material, said powder containing substantially one per cent. to fifteen per cent, available chlo rine, substantially thirty per cent. to ninety per cent. alkali metal compound, and substantially fifteen per cent. to forty per cent. water.

7. A friable alkaline detergent powder comprising a crystalline water-soluble alkaline alkali metal compound containing water of crystallization, a substance selected from the group consisting of kieselguhr and bentonite clay distributed throughout and interspersed between the crystals of said alkaline alkali metal compound, and sodium hypochlorite solution having available chlorine, said hypochlorite solution being absorbed by said water-absorptive material, and said powder containing substantially one per cent. to fifteen per cent. available chlorine, substantially thirty per cent. to ninety per cent. alkali metal compound, and substantially fifteen per cent. to forty per cent. water.

8. A friable alkaline detergent powder comprising a crystalline water-soluble alkaline alkali metal compound containing water of crystallization, a finely-divided solid substantially-inert substantially-Water-insoluble water absorptive material distributed throughout and interspersed between the crystals of said alkaline alkali metal compound, and alkali-metal hypochlorite solution having available chlorine, said hypochlorite solution being absorbed by said water-absorptive material, said powder containing substantially one per cent. to fifteen per cent. available chlorine, substantially thirty per cent. to ninety per cent. alkali metal compound, and substantially fifteen per cent. to forty per cent. water, said water-absorptive material being selected from the group consisting of kieselguhr and bentonite clay.

9. A friable alkaline detergent powder comprising a crystalline watensoluble alkaline alkali metal compound containing water of crystallization, a substance selected from the group consisting of kieselguhr and bentonite clay distributed throughout and interspersed between the crystals of said alkaline alkali metal compound, and sodium hypochlorite solution having available chlorine, said hypochlorite solution being absorbed by said water-absorptive material, said powder containing substantially one per cent. to fifteen per cent. available chlorine, substantially thirty per cent. to ninety per cent. alkali metal compound, and substantially fifteen per cent. to forty per cent. water, said water-soluble alkaline alkali-metal compound being selected from the group consisting of soda ash and trisodium phosphate.

10. A friable alkaline detergent powder substantially free of a water hardening alkaline earth compound comprising about thirty per cent. to ninety per cent. of water-soluble alkaline alkali metal compound, a substance selected from the group consisting of kieselguhr and bentonite clay distributed throughout the particles of said alkaline alkali metal compound, and sodium hypochlorite solution having not more than about fifteen per cent. available chlorine and absorbed by said water-absorptive material to form a friable and dry appearing powder, the ratio of available chlorine to free alkali in said powder being in the neighborhood of one to fifteen.

11. A friable alkaline detergent powder comprising about thirty per cent. to ninety per cent. of a water-soluble alkaline alkali metal detergent material, a substance selected from the group consisiing of kieselguhr and bentonite clay mixed with said alkali metal material, and sodium hypochlorite solution having not more than about fifteen per cent. available chlorine and absorbed by said water absorptive material forming a friable and dry appearing powder, the ratio of available chlorine to free alkali in said powder being in the neighborliddd" oToneTo-fifteeF--1 7vThe process of making an alkaline de- 12. A friable alkaline detergent powder substantially free of water hardening alkaline earth compound comprising a water-soluble crystalline alkaline alkali metal compound, a finely-divided inorganic solid substantially-inert inorganic substantially water-insoluble water-absorptive material distributed throughout and interspersed between the crystals of said alkaline alkali metal compound, and alkali-metal hypochlorite solution having available chlorine, said hypochlorite solution being present in an amount too great to be chemically combined with said alkaline alkali metal compound as water of crystallization to form a dry substantially non-setting powder at ordinary temperatures in the absence of water-absorptive material, and said water-absorptive material carrying mechanically absorbed bypochlorite solution to form a friable dry appearing and substantially non-setting powder, said powder containing substantially one per cent. to fifteen per cent. available chlorine, and substantially thirty per cent. to ninety per cent. crystalline alkaline alkali metal compound, and substantially fifteen per cent. to forty per cent. water.

13. An alkaline detergent powder comprising about fifty-eight per cent. soda ash, about six per cent. silicate of soda, about seven per cent kieselguhr, and sodium hypochlorite solution to give the powder about four per cent. available chlorine and about twenty per cent. water.

14. An alkaline detergent powder comprising about twenty-eight per cent. soda ash, about six per cent. silicate of soda, about twenty-eight per cent. tri-sodium phosphate, about nine per cent, kieselguhr, and sodium hypochlorite solution to give the powder about four per cent. available chlorine and about twenty per cent. water.

15. An alkaline detergent powder comprising about thirty-four per cent. soda ash, about sixteen per cent. tri-sodium phosphate, about four per cent. caustic soda, about six per cent. silicate of soda, about eleven per cent. kieselguhr, and sodium hypochlorite solution to give the powder about four per cent. available chlorine and about twenty per cent. water.

16. The process of making an alkaline detergent powder which comprises passing chlorine into an aqueous solution of caustic soda to form sodium hypochlorite, mixing with said sodium hypochlorite a water soluble alkali metal compound and an inert water absorptive material selected from the group consisting of kieselguhr and bentonite, and introducing gaseous carbon dioxide with the mixture so formed to produce a friable compound.

tergent powder which comprises passing chlorine into an aqueous solution of caustic soda to form sodium hypochlorite, mixing with said sodium hypochlorite a water soluble alkali metal compound, and introducing into the mixture so formed gaseous carbon dioxide to form a friable compound.

ROY C. SUTTON. 

